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By Graham W. Mark

A chemical method of analysis for beryllium was developed recently in Bureau of Mines laboratories. In this method, quinalizarin (1-2-5-8 tetrahydroxyanthraquinone) in N/4 NaOH is used as a colorimetric titration reagent. This solution has a reddish-purple color, whereas the solution containing equivalent amounts of beryllium and the dye is rather blue. In the titration procedure, standard quinalizarin solution is added to the unknown beryllium sample and to two standard beryllium samples of different but known concentrations. Then adjustments in concentrations of BeO in the two known and of quinalizarin in all three are made until the red-violet shade of the unknown is halfway between that of the two knowns. The amount of BeO in the unknown is calculated from the known BeO content of the solutions between which it lies. It is extremely difficult to distinguish the slight differences in shade of these solutions without the use of a proper light filter, especially when the concentration is over 0.1 mg. of BeO, so a study was made of the transmission characteristics of quinalizarin in N/4 NaOH and of the corresponding beryllium complex to determine what filter would give the most contrast.

Jan 1, 1950

By Bernard Lewis

This report summarizes fundamental research and technical studies conducted by the Explosives and Physical Sciences Division of the Bureau of Mines from July 1, 1949, to June 30, 1950. It is the fourteenth of a series of annual reports whose aim has been to bring to the reader a résumé of the research results that have appeared in published form during each fiscal year under the authorship of members of the staff. These are referred to throughout the report.

Jan 1, 1951

By H. Kenworthy

Small batches of fluorspar flotation concentrates were made into nodules and pellets on a laboratory scale. Several of these were rated acceptable by laboratory evaluation methods. The most satisfactory pellets were produced by mixing fluorspar with about 12.5 percent of water, by weight, and 4 percent of organic binders. These binders) for the most part) originated from petroleum and wood-pulp industries. They were generally difficult to handle and were not easily incorporated with the fluorspars tested. Most of them seemed to have an aversion for damp fluorspar and had to be forcibly mixed with the fluorspar; which was then formed into pellets by pressure. Substitution of fuel oil in varying amounts in the binders enhanced the mixing and penetrating qualities of these binders but at the same tire tended to make the pellets more porous. Tall oils performed the same function to a lesser degree and usually decreased the water absorbency of the finished pellets. Heat-treating temperatures to set up these binders were moderate -about 5000 F. for 30 to 50 minutes was usually enough for both drying and heat treating. Nodules made with 1-1/2 to 2 percent of bentonite as a binder were easily mixed and formed. They required a high degree of heat (about 1,500° F.) to develop their strength and were quite water-absorbent when finished. Two fluorspars were examined for weight and fluorite loss after heat treatment at similar temperatures. Both showed a definite wej.ght and analytical loss of fluorite. Bentonite was used also as a binder to successfully nodulize finely ground oxides of iron, manganese, and nickel.

Jan 1, 1951

By W. J. Kroll

This report is concerned with the many sidelines that were investigated incidental to developing a process to produce ductile Zirconium by members of the staff of the Bureau of Mines laboratory, Albany, Oreg. The results of the main investigation, concerning the production of malleable zirconium by reduction of chloride with fused magnesium under helium, have been described in previous publications. These should be taken as a background to facilitate understanding of this work. Literature on the metallurgy of zirconium has been summarized in a separate publication (2), and references are given in this report only when new publications have to be considered or old ones stressed. Most of the observations described in this report can be applied to the problems involved in making titanium with virtually no change. In general, titanium is easier to reduce than zirconium, since its affinities are lower. Also, its chloride is easier to handle and keep clean because it is a liquid at room temperature.

Jan 1, 1952

By Fred D. Wright

This paper describes research at the Bureau of Mines experimental oil-shale mine at Rifle, Colo., to improve blasting techniques and reduce breaking costs. Many of the conclusions are applicable to any mining operation. Experiments Were conducted on many phases of blasting. The effectiveness of various grades of explosives was compared, and several different drill-hole patterns were tried in heading rounds. An experiment was conducted to determine the maximum effective burden for various diameter blast holes. High-speed motion-picture studies were made of blasts, and the time for initial movement of rock after detonation of the explosive was measured. Experiments with millisecond-delay detonators in heading rounds proved that, when used properly, these detonators result in improved fragmentation, economical use of explosive, and compact, easily loaded muck piles.

Jan 1, 1953

By J. R. Thoenen, B. H. Clemmons, A. H. Reed

"INTRODUCTION AND SUMMARYOverall red-ore reserves in the Birmingham, Ala., area were estimated in 1910 by E. F. Burchard 4/. Since then mining has progressed into areas classed by Burchard as ""unavailable for exploitation"" under conditions existing at that time. This is understandable when it is considered that red iron ore was valued at $1.19 a gross ton at the mine in Birmingham in 19102/ and by 1948 had risen 300 percent; 6/ that skips had replaced cars in slope haulage; that mechanical loading and rubber-tired haulage had replaced hand loading and mule or locomotive haulage; and that other more efficient mining methods had been introduced. Intensive study during the intervening 40 years has been given to ways and means for upgrading the low-grade ores in the area and combining or blending them with raw red and brown ores for improved blast-furnace feed.It is reasonable to expect that future progress in mining efficiency and increased knowledge of the beneficiation characteristics of marginal ores will permit extraction of red-iron minerals now considered uneconomic.The Bureau of Mines has undertaken to restudy iron-ore reserves of the Birmingham area to determine what tonnage and grades of mineral are present; what is necessary to make them amenable to mining; what further advancement is possible in beneficia¬tion methods; and where increased production may be obtained in the area if and when required. This study has been underway for the past 2 years, but research into the beneficiation of marginal ores has been in progress at the Southern Experiment Station for the past 30 years. Many results of that research have been adopted in commercial practice in the area. Other results have not been published but are pre¬sented here in condensed form as an important factor in assessing marginal deposits with respect to their importance as ore reserves.An interim discussion of the salient features of past history and progress, as well as the data developed during the years of research in beneficiation at this station and the present field investigation, will make for a better understanding of the present position as well as be useful in evaluating future potentialities. Discussion in this paper is confined to the main Birmingham Basin area, which contains the largest concentration of hematite ores in the district."

Jul 1, 1953

By J. F. Barkley

Two major problems in the operation of air preheaters for boilers are corrosion and the accumulation of deposits on the heating surfaces. Corrosion or loss of metal necessitates replacement of parts; the accumulation of deposits decreases the size of the gas and air passages, resulting in increased pressure drop for the same gas flow, and also affects the heat transfer. These items, either singly or together, limit the capacity and efficiency at which the equipment can be operated and affect its availability, even causing undesirable shutdowns under extreme conditions The field and laboratory work on regenerative air preheaters described in this report covers research on the relative corrosion resistance of different materials, such as various metals, special metal coverings, and fired clays, and studies on deposits, their nature, analyses, and corrosive effects. This is the first report on cooperative work of The Air Preheater Corp., of New York City, and the Federal Bureau of Mines.

Jan 1, 1953

By Bernard Lewis

This report summarizes fundamental research end technical studies conducted in the Explosives and Physical Sciences Division, Region VIII, of the Bureau of Mines in the 2 years July l, 1950, to June 30, 1952. It is the fifteenth of a series of, ordinarily, annual reports whose aim has been to provide the reader with a resume of the research results that have appeared in published form during each fiscal year under the authorship of members of the staff. These are referred to throughout the report. ACKNOWLEDGMENTS Acknowledgments art, made to the following members of the Division wider whose mediate supervision the described studies were carried out. Stuart R. Brinkley, Jr., chief, Mathematical and Theoretical Physics Section, and special assistant to the chief of the division.

Jan 1, 1953

By R. T. MacMillan

A number of chemical techniques have been applied to manganese ores from three areas of Aroostook County, Maine. Although large tonnages of these ores have been proved, they are low grade, and their exploitation has awaited a suitable beneficiation scheme. As conventional ore-dressing methods had failed to yield satisfactory results, attention was turned to chemical procedures. Leaching with dilute (7-percent) H2S04 extracted over 90 percent of the manganese from ore of the Dudley farm area, consuming 3.8 pounds of acid per pound of manganese extracted. Ores from the Littleton Ridge and Maple Mountain-Hovey Mountain areas were less amenable to this treatment, yielding approximately 80 and 60 percent of their Mn content, respectively. To increase the percentage extraction of manganese in the latter two ores, a number of factors were varied, including (1) acid concentration in the extracting solution, (2) ratio of acid to Mn in the slurry, and (3) preliminary heat treatment of the ore with a reducing agent. Other acids, including HNO3, HC1, and H2SO3, were tried also; however, no significant improvements in the Mn leached from Maple Mountain-Hovey Mountain ore were made. The manganese extraction of Littleton Ridge ore was raised to 90 percent by providing 9 to 11 pounds of HNO3 per pound of Mn in the ore.

Jan 1, 1954

By John P. Walsted

Because of the absence of an iron-producing industry, the Pacific Northwest is working under an economic handicap. This is particularly apparent in the gray-iron-foundry industry because of the high price of pig iron imported from foreign sources or shipped in from producing ?areas within the United States. The high prices and sometimes short supply of ferrous metal products has put a brake on industrialization, which has been only partly compensated by the availability of cheap electric power. The economic condition of the gray-iron-foundry industry could be improved by establishing a small iron-producing industry based on the locally available ores. Moreover, establishing a local iron smelter would create a market for resources now dormant. Low-grade ores of manganese, chromium, and nickel would become usable in industry when combined with the iron ore from Scappoose. Pig iron produced in even limited quantities would level out the fluctuation in supply. The ore deposits, being small, would not supply enough pig iron to satisfy the entire demand. This condition necessitates designing special pig irons that will carry abnormally high proportions of scrap in the cupola charge.

Jan 1, 1955

By C. C. Popoff

The growth of the aluminum-smelting industry in the Pacific Northwest, resulting from national defense requirements, emphasized a need for local sources of alumina to supplement the alumina production shipped from the East. Because supplies of foreign bauxite were being interrupted and our domestic bauxite reserves were inadequate, it was necessary to expedite the investigation of other possible sources of alumina during World War II. A program of investigation of high-alumina clay deposits in the Northwest was carried out jointly by the Federal Geological Survey and the Federal Bureau of Mines. As part of this program the Cowlitz clay deposits near Castle Rock, Wash., were explored by the Bureau of Mines in 1942-43. These deposits are near railroads, tide-water, and Bonneville Power Administration lines and within 22 to 100 miles of 4 aluminum-reduction plants.

Jan 1, 1955

By M. J. Spendlove

A progress report is presented on a research program in which an attempt was made to develop a practical sulfide-volatilization process for recovering tin from low-grade Bolivian ores. Shaft-furnace designs and operating techniques were studied in a series of experiments in which the objective was to sulfidize cassiterite to stannous sulfide, remove the stannous sulfide by volatilization, reconvert the stannous sulfide to stannous oxide, and collect the resulting fume. A shaft furnace was developed and operated in a final test in which many of the previous difficulties were surmounted. Since the supporting funds were exhausted at this point, the project was discontinued; recommendations for further improvements in furnace design and operation were made on the basis of interpretation of experimental results obtained in shaft-furnace experiments and other related studies.

Jan 1, 1955

By T. T. Campbell

Although secondary recovery of lead and lead-tin alloys has been common practice in the United States during recent years, there is little published in-formation concerning recovery techniques. Available information does not cover metal recovery from wet dross skimmings. This investigation by the Bureau of Mines was undertaken to develop techniques that would allow lead-tin alloys to be recovered from wet dross skimmings containing large amounts of zinc chloride. A process was developed, on a laboratory scale, for recovering lead-tin alloys from wet solder dross skimmings. Straight water leaching, either with or without a second leaching operation carried out with a Na2C03 addition for removing chloride, produced a dross that could be smelted without further treatment. Overall recoveries averaging 92 percent of the metal values in the dross were obtained in the form of lead-tin alloys, which had an average tin content of 16 percent and lead content of 84 percent. The recovered alloy contained less than 0.02 percent zinc, as determined by both chemical and spectrographic analyses.

Jan 1, 1956

By M. M. Fine

A preliminary mineral-dressing study of five samples of East Texas limonitic brown iron ores was conducted as part of the Bureau of Mines program to develop and extend domestic resources of iron ore. The samples were considered to be typical of ore currently being mined and beneficiated by the Lone Star Steel Co. and Sheffield Steel Co. The objective of the research was to investigate those mineral-dressing unit operations that might recover some of the fine iron lost in current industrial wastes or perhaps improve the recoveries when applied to the ores as well. Since current industrial beneficiation practice yields a washed limonite analyzing 41 to 45 percent iron, higher grade concentrates were not sought in this laboratory study. Laboratory investigation included washing and sizing, reduction roasting, and subsequent magnetic separation of the finely ground roasted materials. The results showed that laboratory recoveries of over 80 percent of the iron were possible, for the ores investigated, at concentrate grades comparable to those expected from cur-rent industrial beneficiation practice. ACKNOWLEDGMENTS Acknowledgment is made to the Lone Star Steel Co. and Sheffield Steel Co. for supplying the brown iron-ore samples on which this research was conducted.

Jan 1, 1956

By F. E. Block

The reaction between calcined dolomite and ferrosilicon has been studies with the aim of developing a continuous process for magnesium production. Small-scale tests were made in vacuum retorts similar to those used in the vacuum retort process as developed by Pidgeon (1)2/ and operated during the period of World War II in several Government-owned plants. Factors investigated with respect to the silicon efficiency were the reaction temperature, reaction time, amount of excess dolomite in the charge, and effect of adding sodium silicate to the charge to serve as a binder. Additional laboratory tests were made to study the reaction at elevated temperature but at atmospheric pressure. Silicon efficiencies exceeding 80 percent were found to result when operating in the temperature range from 1,750° to 1,800° C. for periods of 20 to 30 minutes.

Jan 1, 1956

By J. R. Nettle

A method has been developed in the laboratory for successfully electro-refining titanium metal. Refining is accomplished in e fused-salt electrolyte using offgrade metal as the anode and collecting the purified metal at the cathode. The characteristics and requirements of the various alkali chlorides tested as electrolytes are discussed in relation to relative ease of purification and serviceability. The various types of cells designed and tested for electrorefining are illustrated and their method of operation discussed. The individual advantage of each cell and the purpose for which it was designed are reviewed. The magnitude of the cathode current density was found to depend largely upon the quantity of soluble titanium chloride in the electrolyte. The physical condition of the anode also greatly affected the cathode current density.

Jan 1, 1957

By R. R. May

A preliminary examination of the Houston strip-coal mine, situated on the Alaska Railroad at milepost 175 (61 rail miles north of Anchorage, Alaska) and a review of all available information resulting from early coal exploration activities in the area resulted in plans to investigate the coal-bearing formations at depth by means of diamond core drilling to indicate the existence of additional reserves of coal in close proximity to railroad transportation, where it would be quickly available to meet rapidly expanding military and civilian fuel requirements. From the date of mobilization of equipment, August 28, 1951, until date of suspension, August 18, 1952, 2,010 feet of diamond drilling was completed. Ten definable coal beds were cut, of which 2 appear to be persistent and minable over an area of approximately 1/2 square mile. Within this area the 2 minable beds contain approximately 5,000,000 tons of coal in place. Of the remaining beds, at least two others may be minable to the eastward near their projected outcrops; however, these and deeper beds (at least in the vicinity of the drill holes) lie beneath a zone of pressurized gas and brackish water. From a practical standpoint, continued development and utilization of the coal in this vicinity will depend on the operators' ingenuity in developing cheap mining methods and on diligent prospecting for strippable coal under the comparatively light glacial cover.

Jan 1, 1957

By Carl Rampacek, W. A. McKinney

The feasibility of leaching calcareous and siliceous oxidized copper ores by downward percolation with dilute acid was investigated in the laboratory and in a small continuous plant operated by the Federal Bureau of Mines . The crushed ore was leached in deep columns with solutions containing 1 or 5 percent sulfuric acid to dissolve the oxidized copper . Bench - scale laboratory tests on two calcareous ores from the same deposit indicated that a maximum copper extraction , about 72 percent , could be expected from heap leaching a feed as coarse as 1 inch . Laboratory tests on a siliceous ore showed that almost 70 percent of the copper could be extracted by leaching a 1 / 4 - inch feed . The bench - scale tests were supplemented by larger continuous runs wherein the copper was recovered from the leach liquors by precipitation on detinned scrap iron . Leaching the calcareous ore for approximately 10 days recovered 62 percent of the total copper . The sulfuric acid consumption was 9.6 pounds per pound of copper recovered . Treatment of the siliceous ore recovered 62.5 percent of the total copper in a 2.5 - day leach and the acid consumption was 3.7 pounds per pound of copper recovered . Cement copper products that assayed over 71 percent copper were obtained from the leach solutions by precipitation on scrap iron . The bench - scale and continuous tests demonstrated that downward percolation leaching of the calcareous ores was technically feasible but not economically practicable because of high acid consumption by the gangue . Leaching of the siliceous ore was rapid and the acid and water requirements were nominal . The downward percolation leach procedure is simple and requires a minimum of plant equipment .

Jul 1, 1960

By A. L. Engel

This publication describes further research by the Federal Bureau of Mines in beneficiating domestic manganese ores. The ores selected for treatment were typical of many manganese deposits in California and Nevada in that they have not been economical to mine because they are low grade or contaminated with siliceous minerals and are not amenable to physical concentration.3 4/ It would be desirable to develop a simple treatment method resulting in nearly complete extraction of manganese from these ores and applicable to small-scale operations. Sulfation reduction appeared to be such a method. The studies reported in this publication were directed toward sawdust or lignin-sulfonates as reducing agents. Sawdust, as waste from lumbering, and lignin-sulfonates, byproducts of woodpulp papermaking, are comparatively cheap and may be available in areas where manganese ores are found. Sugar, oils, and coal were also tried as reducing agents.

Jan 1, 1960

By H. F. Yancey

Traditionally the Pacific Northwest has relied on hydroelectric power, which has been both abundant and cheap. However, comparatively few hydroelectric sites capable of providing low-cost power remain, therefore the need for supplemental thermal generation, perhaps within the next decade, is generally recognized. Based on the present cost and availability of competing fuels, coal seems to be the logical choice for projected thermal power plants. Power companies and public utilities have become interested in establishing reserves of coal for future use. One deposit explored in 1958-59 lies in southern Thurston and northern Lewis Counties, Wash., near Centralia. Drilling, totaling 22,700 feet, proved the existence of 70 million tons of strippable coal--an ample reserve for the projected power plant. The coal, like most others and particularly those of Washington and Oregon, when mined in full seam section by mechanical methods, would require cleaning to make it suitable for use. The amount and nature of the impurities in this coal dictated a thorough investigation of its cleaning characteristics to establish economic factors and to insure proper preparation-plant design. Therefore, arrangements were made through a cooperative agreement to conduct such work at the Seattle Coal Research Laboratory of the Bureau of Mines. This report describes that investigation. The results are of interest primarily in connection with the utilization of this particular deposit, but some of the information developed is applicable to other deposits of low-rank coals in the West, because the impurities in these coals differ greatly in behavior from those generally associated with the higher rank coals of the Appalachian field.

Jan 1, 1961